Search Results (202)

A review of studies has shown that aromatic azo and hydrazo derivatives are used in a wide spectrum of fields, including food, pharmaceutical, and cosmetic products, as well as in technical and electronic technologies, which has contributed to the development of new such compounds. In this work, the structures of newly obtained 4-methyl-3,5-dinitro-2-(2-phenylhydrazinyl)pyridine (4MDNPHP) and its azo derivative, 4-methyl-3,5-dinitro-2-[(E)-phenyldiazenyl]pyridine (4MDNPAP), were established by spectroscopic (NMR, IR, Raman, and UV-Vis) and emission studies. Single-crystal X-ray diffraction analysis was used to determine the molecular structure of the studied compounds, and the results were compared with DFT calculations (B3LYP/6-311G(2d,2p)). The collected X-ray data revealed that the crystal of the hydrazo compound (4MDNPHP) belongs to the triclinic space group P$\overline{1}$ (Z = 2), whereas the crystal of the azo compound (4MDNPAP) follows the symmetry of the monoclinic space group P2₁/n (Z = 4). Both presented derivatives crystallized with one molecule in the asymmetric unit. Specific properties of the hydrazo bridge C_ϕ-NH-NH-C_θ moiety and its azo counterpart C_ϕ-N=N-C_θ were considered in detail. Full article

This study systematically investigates the effect of hydrogen flow rate (100, 200, 300, and 400 sccm) on the properties of DC53 steel during a 4 h plasma nitriding process conducted at 400 °C in an asymmetric bipolar pulsed reactor. A comprehensive characterisation approach was employed. X-ray diffraction (XRD) was used to identify the phase composition, revealing the formation of a compound layer consisting of ε-Fe_2–3N (identified by its (100), (101), and (102) planes) and γ’-Fe₄N (identified by its (220) plane). Mechanical properties were assessed using Vickers microhardness for surface measurements and nanoindentation for depth profiling. Glow discharge optical emission spectroscopy (GD-OES) provided elemental depth analysis, while a ball-on-disk tribometer evaluated the tribological performance. The optimal treatment was achieved at a hydrogen flow rate of 200 sccm. This condition yielded a peak surface hardness of 1121.5 ± 69.2 HV_0.2. GD-OES analysis directly correlated this mechanical enhancement to a high surface nitrogen content of approximately 8.5% and an effective diffusion depth of about 50 µm. Full article

Rare-earth oxides possess distinctive electronic configurations, tunable oxidation states, and inherent structural robustness, making them highly attractive for advanced energy storage applications. Among these, neodymium oxide (Nd₂O₃) stands out due to its high surface redox activity, structural stability, and favorable band alignment, enabling efficient charge storage in electrochemical devices. In this study, Nd₂O₃ electrodes were synthesized via a sol–gel method with systematically varied precursor concentrations (1 mM, 3 mM, and 5 mM) to elucidate the impact of synthesis on crystallinity, morphology, and electrochemical performance. X-ray diffraction (XRD) confirmed the formation of the hexagonal Nd₂O₃ phase, with the 3 mM sample (Nd-2) exhibiting the sharpest reflections, indicative of enhanced crystallinity and reduced lattice defects. X-ray photoelectron spectroscopy (XPS) revealed trivalent Nd species and both lattice and surface oxygen, providing abundant redox-active sites. Field Emission Scanning Electron Microscope (FE-SEM) showed Nd-2 possessed a hierarchically interconnected fibrous network decorated with fine granules, maximizing active surface area and facilitating rapid ion diffusion. Electrochemical testing demonstrated that Nd-2 achieved an areal capacitance of 20 F cm⁻², a diffusion-controlled pseudocapacitive contribution of ~84.9%, and retained 86.3% capacitance over 12,000 cycles. An asymmetric supercapacitor with Nd-2 and activated carbon delivered an energy density of 0.132 mWh cm⁻², power density of 1.8 mW/cm², and 81.1% capacitance retention over 7000 cycles. These results highlight the critical role of precursor concentration in tailoring structure and electrochemical performance, establishing Nd₂O₃ as a promising electrode for high-performance energy storage devices. Full article

This study successfully produced a magnesium alloy bar featuring a bimodal microstructure with high strength via an asymmetric upsetting–extrusion process. The evolution of microstructure, texture, and mechanical properties was systematically investigated using finite element simulation, room-temperature tensile tests, optical microscopy, scanning electron microscopy, and electron backscatter diffraction. Results demonstrate that the bimodal structure forms under the combined effects of shear deformation in the upsetting stage and low-speed, high-ratio deformation in the extrusion stage. This structure consists of coarse deformed grains containing high-density dislocations surrounded by fine dynamically recrystallized grains. A strong <10-10>//ED basal fiber texture also developed, which effectively suppresses basal slip. Continuous dynamic recrystallization was the primary grain refinement mechanism. The 370 °C extruded alloy achieved a high tensile strength of 457.9 MPa, but its elongation was limited to 3.96%. This combination of strength and ductility is attributed to the synergistic influence of the bimodal microstructure, strong basal texture, and high dislocation density. Full article

The rational design of transition metal oxides with tailored electronic structures and defect chemistries is critical for advancing high-performance supercapacitors. Herein, we report the engineering of cobalt oxide (Co₃O₄) gels through controlled sol–gel synthesis and rare earth (RE) incorporation using neodymium (Nd), gadolinium (Gd), and dual neodymium/gadolinium (Nd/Gd) doping. X-ray diffraction (XRD) confirmed the preservation of the cubic spinel structure with systematic peak shifts and broadening, evidencing lattice strain, oxygen vacancy generation, and defect enrichment. Field-emission scanning electron microscopy (FE-SEM) analyses revealed distinct morphological evolution from compact nanoparticle assemblies in pristine Co₃O₄ to highly porous, interconnected frameworks in Nd/Gd–Co₃O₄ (Nd/Gd-Co). X-ray photoelectron spectroscopy (XPS) verified the stable incorporation of RE ions, accompanied by electronic interaction with the Co–O matrix and enhanced oxygen defect states. Electrochemical measurements demonstrated that the Nd/Gd–Co electrode achieved a remarkable areal capacitance of 25 F/cm² at 8 mA/cm², superior ionic diffusion coefficients, and the lowest equivalent series resistance (0.26 Ω) among all samples. Long-term cycling confirmed 84.35% capacitance retention with 94.46% coulombic efficiency after 12,000 cycles. Furthermore, the asymmetric pouch-type supercapacitor (APSD) constructed with Nd/Gd–Co as the positive electrode and activated carbon as the negative electrode delivered a wide operational window of 1.5 V, an areal capacitance of 140 mF/cm², an energy density of 0.044 mWh/cm², and 89.44% retention after 7000 cycles. These findings establish Nd/Gd-Co gels as robust and scalable electrode materials and demonstrate that RE co-doping is an effective strategy for bridging high energy density with long-term electrochemical stability in asymmetric supercapacitors. Full article

Crystal molecular structure of 3-(anthracen-2′-yl)-ortho-carborane was determined by single crystal X-ray diffraction study at 100 K. The asymmetric cell unit contains two enantiomeric pairs of molecules, in one of which the intramolecular dihydrogen bond CH...HB is formed with the participation of the C(1)H hydrogen of the anthracene substituent, and in the other with the participation of the C(3)H hydrogen. In all molecules, the polycyclic aromatic and carborane fragments are rotated relative to each other in such a way that the C-C bond of the ortho-carborane cage is approximately parallel to the plane of the aromatic substituent. According to quantum chemical calculations, the minimum energy corresponds to the formation of an intramolecular dihydrogen bond C(1)H...HB(4/7), whereas the C(3)H...HB(4/7) bond is formed rather as a result of intermolecular interactions in the crystal lattice. Full article

(±)-tiaprofenic acid (TA), marketed as (Surgam^®), belongs to the family of NSAIDs, with the peculiarity of a reduced incidence of ulcer induction in rats compared with parent drugs. However, some adverse effects were observed, and better knowledge of its interaction with biologic substrates is needed. Unfortunately, unlike most commercial NSAIDs, suitable single crystals for an X-ray diffraction study could not be obtained. To fill the gap, the crystal structure of TA was solved by X-ray powder diffraction, and the molecular interactions stabilizing the structure were analyzed by Hirshfeld surface and energy framework analysis. TA crystallizes in the $P{2}_1/c$ space group, with its two enantiomers in the asymmetric unit, further confirming the peculiarity of the crystal structure and the difficulty of solving it. TA packing is characterized by alternating enantiomers connected through hydrogen bonds, forming chains, arranged in layers, stabilized by $\pi$-stacking. First principle modeling revealed several stable conformations within 4$\mathrm{k}$$\mathrm{J}$ ${\mathrm{mol}}^{-1}$ of the global minimum and the relaxed potential energy scans revealed modest (8$\mathrm{k}$$\mathrm{J}$ ${\mathrm{mol}}^{-1}$ to 15$\mathrm{k}$$\mathrm{J}$ ${\mathrm{mol}}^{-1}$) energy barriers. Such flat energy landscape suggests flexible and dynamic behavior of tiaprofenic acid in solution and in vivo conditions, with multiple suitable docking sites. Full article

We report here an in-depth study concerning the synthesis, NMR, and X-ray structure determination of two new polymorphs of 2-chloro-3′,4′-diacetoxy-acetophenone. A new, ecologically friendly method of synthesis in the solid phase, as well as a suitable method for protecting hydroxyl functionality, is presented. The ¹H- and ¹³C-NMR spectra as well as the single crystal X-ray diffraction studies proved unambiguously the structure of the compounds: the two polymorphs of 2-chloro-3′,4′-diacetoxy-acetophenone and 2-chloro-3′-hydroxy-4′-acetoxy-acetophenone. The polymorph I crystalizes in the monoclinic P21/c space group, while polymorph II crystalizes in the Sohnke P212121 space group of the orthorhombic system, with no interstitial solvate molecules. Significant differences were observed in the supramolecular interactions in the crystal structure of the two polymorphs. Polymorph I is characterized as a parallel packing of weakly interacting supramolecular layers oriented in the 1 1 0 plane. The crystal structure of polymorph II is much more complex: each molecule is interconnected through 12 (twelve) hydrogen bonds with 9 (nine) adjacent symmetry-related molecules. The monoacetoxy derivative 2-chloro-3′-hydroxy-4′-acetoxy-acetophenone 3 crystallizes in the monoclinic P2₁/c space group, with one molecule in the asymmetric unit. Full article

A para-substituted 1,10-phenanthroline ligand, 2-(4-methylphenoxy)-1,10-phenanthroline (L24), was synthesized and structurally characterized. Complexes with Eu³⁺, Tb³⁺, Sm³⁺, and Dy³⁺ were obtained in a 2:1 ligand-to-metal ratio and analyzed using single-crystal x-ray diffraction, photoluminescence spectroscopy, and TD-DFT calculations. Coordination via the phenanthroline nitrogen atoms, combined with steric asymmetry from the para-methylphenoxy group, induces low-symmetry environments favorable for electric-dipole transitions. Excited-state lifetimes reached 2.12 ms (Eu³⁺) and 1.12 ms (Tb³⁺), with quantum yields of 42% and 68%, respectively. The triplet-state energy of L24 (22,741 cm⁻¹) aligns well with emissive levels of Eu³⁺ and Tb³⁺, consistent with Latva’s criterion. Fluorescence titrations indicated positively cooperative complexation, with association constants ranging from 0.60 to 1.67. Stark splitting and high ⁵D₀ → ⁷F₂/⁷F₁ intensity ratios (R₂ = 6.25) confirm the asymmetric coordination field. The para-methylphenoxy substituent appears sufficient to lower coordination symmetry and strengthen electric-dipole transitions, offering a controlled route to enhance photoluminescence in Eu³⁺ and Tb³⁺ complexes. Full article

Asphalt plant reclaimed powder is a common solid waste in road engineering. Reusing reclaimed powder as filler holds significant importance for environmental protection and resource conservation. The key factors affecting the feasibility of reclaimed powder reuse are its acidity/alkalinity and cleanliness. Traditional evaluation methods, such as the methylene blue test and plasticity index, can assess reclaimed powder properties to guide its recycling. However, these methods suffer from inefficiency, strong empirical dependence, and high variability. To address these limitations, this study proposes a rapid and precise evaluation method for reclaimed powder properties based on Fourier transform infrared spectroscopy (FTIR). To do so, five field-collected reclaimed powder samples and four artificial samples were evaluated. Scanning electron microscopy (SEM), X-ray fluorescence spectroscopy (XRF), and X-ray diffraction (XRD) were employed to characterize their microphase morphology, chemical composition, and crystal structure, respectively. Subsequently, FTIR was used to establish correlations between key acidity/alkalinity, cleanliness, and multiple characteristic peak intensities. Representative infrared characteristic peaks were selected, and a quantitative functional group index (Is) was proposed to simultaneously evaluate acidity/alkalinity and cleanliness. The results indicate that reclaimed powder primarily consists of tiny, crushed stone particles and dust, with significant variations in crystal structure and chemical composition, including calcium carbonate, silicon oxide, iron oxide, and aluminum oxide. Some samples also contained clay, which critically influenced the reclaimed powder properties. Since both filler acidity/alkalinity and cleanliness are affected by clay (silicon/carbon ratio determining acidity/alkalinity and aluminosilicate content affecting cleanliness), this study calculated four functional group indices based on FTIR absorption peaks, namely the Si-O-Si stretching vibration (1000 cm⁻¹) and the CO₃²⁻ asymmetric stretching vibration (1400 cm⁻¹). These indices were correlated with conventional testing results (XRF for acidity/alkalinity, methylene blue value, and pull-off strength for cleanliness). The results show that the Is index exhibited strong correlations (R² = 0.89 with XRF, R² = 0.80 with methylene blue value, and R² = 0.96 with pull-off strength), demonstrating its effectiveness in predicting both acidity/alkalinity and cleanliness. The developed method enhances reclaimed powder detection efficiency and facilitates high-value recycling in road engineering applications. Full article

To develop high-performance electrode materials for supercapacitors, in this paper, a heterostructured composite material of cerium sulfide and zinc sulfide quantum dots (CeS₂/ZnS QD) was successfully prepared by hydrothermal method. Characterization through scanning electron microscopy (SEM), X-ray diffraction (XRD), and transmission electron microscopy (TEM) showed that ZnS QD nanoparticles were uniformly composited with CeS₂, effectively increasing the active sites surface area and shortening the ion diffusion path. Electrochemical tests show that the specific capacitance of this composite material reaches 2054 F/g at a current density of 1 A/g (specific capacity of about 256 mAh/g), significantly outperforming the specific capacitance of pure CeS₂ 787 F/g at 1 A/g (specific capacity 98 mAh/g). The asymmetric supercapacitor (ASC) assembled with CeS₂/ZnS QD and activated carbon (AC) retained 84% capacitance after 10,000 charge–discharge cycles. Benefited from the synergistic effect between CeS₂ and ZnS QDs, the significantly improved electrochemical performance of the composite material suggests a promising strategy for designing rare-earth and QD-based advanced energy storage materials. Full article

The flexible transparent conductive films (TCFs) of a ZnS/Cu/Ag/TiO₂ multilayered structure were deposited on a flexible PET substrate with high surface roughness using magnetic sputtering, and the effects of structural characteristics on the performance of the films were analyzed. The TCFs with TiO₂/Cu/Ag/TiO₂ and ZnS/Cu/Ag/ZnS symmetric structures were also prepared for comparison. The TCF samples were deposited using ZnS, TiO₂, Cu and Ag targets, and they were analyzed using scanning electronic microscopy, atomic force microscopy, grazing incidence X-ray diffraction, spectrophotometry and a four-probe tester. The TCFs exhibit generally uniform surface morphology, excellent light transmittance and electrical conductivity with optimized structure. The optimal values are 84.40%, 5.52 Ω/sq and 33.19 × 10⁻³ Ω⁻¹ for the transmittance, sheet resistance and figure of merit, respectively, in the visible spectrum. The satisfactory properties of the asymmetric multilayered TCF deposited on a rough-surface substrate should be mainly attributed to the optimized structure parameters and reasonable interfacial compatibilities. Full article

In industrial applications, rolling is commonly performed with lubrication to prevent undesirable modification of the sheet. Although it is well established that lubrication influences the microstructure and texture of deformed sheets through its effect on shear deformation, the underlying mechanisms remain insufficiently understood. In this study, we investigated how lubrication affects slip system activity during asymmetrical rolling, using viscoplastic modeling of BCC ferritic steel. Two conditions—lubricated and non-lubricated samples—were examined under asymmetrical rolling. Slip system activity was inferred from the rotation axes between pairs of orientations separated by low-angle grain boundaries, based on the assumption that such boundaries represent the simplest form of orientation change. A Viscoplastic Self-Consistent (VPSC) model employing an affine linearization scheme was used. This proved sufficient for evaluating slip system activity in BCC polycrystalline metals undergoing early-stage plastic deformation involving either plane strain or combined plane strain and shear. The results demonstrated that lubrication had a limiting effect by reducing the penetration of shear deformation through the thickness of the sample. Understanding this effect could enable the optimization of lubrication strategies—not only to minimize defects such as bending, but also to achieve microstructural characteristics favorable for industrial applications. Full article

The Campylobacter genus includes many pathogenic species, with Campylobacter hepaticus primarily implicated in spotty liver disease in poultry. Chemotaxis is one of the well-established mechanisms of pathogenesis of Campylobacter. The chemoreceptor Tlp3, previously studied in C. jejuni, mediates responses to diverse ligands. Differences between the ligand-binding pockets of Tlp3s in C. hepaticus and C. jejuni may influence ligand specificity and niche adaptation. Here, we report a method for production of the ligand-binding domain of C. hepaticus Tlp3 (Ch Tlp3-LBD) in Escherichia coli inclusion bodies that yields crystallisable protein. Size-exclusion chromatography analysis showed Ch Tlp3-LBD is a monomer in solution. Ch Tlp3-LBD was crystallised using PEG 6000 and LiCl as the precipitants. The crystal lattice symmetry was P222₁, with unit cell geometry of a = 82.0, b = 137.7, c = 56.1 Å, and α = β = γ = 90°. X-ray diffraction data have been acquired to 1.6 Å resolution using synchrotron radiation. Estimation of the Matthews coefficient (V_M = 2.8 ų Da⁻¹) and the outcome of molecular replacement suggested the asymmetric unit is composed of two protein molecules. This work lays the foundation for studies towards understanding the structural basis of ligand recognition by C. hepaticus Tlp3 and its role in pathogenesis. Full article

This study employed a simple and cost-effective method for developing NiO with reduced optical band gaps that can be combined with nanostructured polyaniline (PANI). The composite systems were used as electrocatalytic and electrode materials in oxygen evolution reactions (OER) and in supercapacitor applications. We prepared the composite material in two stages: NiO was prepared with a reduced optical band gap by combining it with wheat peel extract. This was followed by the incorporation of PANI nanoparticles during the chemical oxidation polymerization process. A variety of structural characterization techniques were employed, including scanning electron microscopy (SEM), powder X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, UV-visible spectroscopy, and X-ray photoelectron spectroscopy (XPS). A surface-modified NiO/PANI composite with enhanced surface area, fast charge transfer rate, and redox properties was produced. When NiO/PANI composites were tested in KOH electrolytic solution, 0.5 mL of wheat peel extract-mediated NiO/PANI demonstrated excellent electrochemical performance. It was found that the asymmetric supercapacitor (ASC) device had the highest specific capacitance of 404 Fg⁻¹ at a current density of 4 Ag⁻¹. In terms of energy density and power density, the ASC device was found to have 140 Whkg⁻¹ and 3160 Wkg⁻¹, respectively. The ASC device demonstrated excellent cycling stability and charge storage rates, with 97.9% capacitance retention and 86.9% columbic efficiency. For the OER process, an overpotential of 320 mV was observed at a current density of 10 mA/cm². It was found that the NiO/PANI composite was highly durable for a period of 30 h. A proposed hypothesis suggested that reducing the optical band gap of NiO and making its composites with PANI could be an appealing approach to developing next-generation electrode materials for supercapacitors, batteries, and fuel cells. Full article